色谱

色谱 ›› 2015, Vol. 33 ›› Issue (1): 22-28.DOI: 10.3724/SP.J.1123.2014.07006

• 研究论文 • 上一篇    下一篇

基于诊断离子策略的超高压液相色谱-线性离子阱-轨道离子阱质谱联用技术解析中药虎杖的化学成分

潘智然1, 梁海龙1, 梁朝晖1, 徐文1,2   

  1. 1. 广州中医药大学第二临床医学院, 广东 广州 510006;
    2. 广东省中医药科学院, 广东 广州 510006
  • 收稿日期:2014-07-02 修回日期:2014-09-16 出版日期:2015-01-08 发布日期:2014-12-26
  • 通讯作者: 徐文
  • 基金资助:

    国家自然科学基金项目(81402887);2012年广州中医药大学优秀青年学者科研基金(No.10);广东省中医药局建设中医药强省科研课题(20121198).

An ultra-high-pressure liquid chromatography/linear ion trap-Orbitrap mass spectrometry method coupled with a diagnostic fragment ions-searching-based strategy for rapid identification and characterization of chemical components in Polygonum cuspidatum

PAN Zhiran1, LIANG Hailong1, LIANG Chaohui1, XU Wen1,2   

  1. 1. The Second College of Clinic Medicine, Guangzhou University of Chinese Medicine, Guangzhou 510006, China;
    2. Guangdong Province Institute of Chinese Medicine, Guangzhou 510006, China
  • Received:2014-07-02 Revised:2014-09-16 Online:2015-01-08 Published:2014-12-26

PDF

403

被引次数

17

摘要：

建立了基于超高压液相色谱-电喷雾-高分辨质谱联用技术(UHPLC-ESI-HRMS)的中药虎杖化学成分的快速定性分析方法.采用Waters UPLC C18色谱柱,乙腈-甲酸水系统梯度洗脱,采用ESI-LTQ-Orbitrap高分辨杂交质谱技术负离子采集,线性离子阱质谱进行多级质谱碎裂,轨道离子阱高分辨检测,获取多维质谱数据.利用代表性成分的诊断离子进行搜寻,结合质谱偶电子规律、氮规律、不饱和度和同位素峰等信息,参阅文献,总结主要成分的裂解规律,对主要峰进行指认与鉴定.结果显示,整个分析过程在10 min内完成,该方法分离良好,灵敏度高.对虎杖根中的34种成分进行了结构分析,研究从中药虎杖中发现了多种酚酸取代二苯乙烯苷、酚酸取代蒽醌苷和蒽醌硫酸盐衍生物等成分.研究结果表明本方法为虎杖的后续化学成分研究、相关产品的质量控制和药效物质基础的研究提供了一种高效、可靠的检测手段.

关键词: 超高压液相色谱, 虎杖, 化学成分, 线性离子阱-轨道离子阱质谱, 中药

Abstract:

A method for qualitative analysis of constituents in Polygonum cuspidatum by ultra-high-pressure liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry (UHPLC-LTQ-Orbitrap MS) has been established. The methanol extract of Polygonum cuspidatum was separated on a Waters UPLC C18 column using acetonitrile-water (containing formic acid) eluting system and detected by LTQ-Orbitrap hybrid mass spectrometer in negative mode. The targeted components were further fragmented in LTQ and high accuracy data were acquired by Orbitrap MS. The summarized fragmentation pathways of typical reference components and a diagnostic fragment ions-searching-based strategy were used for detection and identification of the main phenolic components in Polygonum cuspidatum. Other clues such as nitrogen rule, even electron rule, degree of unsaturation rule and isotopic peak data were included for the structural elucidation as well. The whole analytical procedure was within 10 min and more than 30 components were identified or tentatively identified. This method is helpful for further phytochemical research and quality control on Polygonum cuspidatum and related preparations.

Key words: Polygonum cuspidatum, chemical components, LTQ-Orbitrap mass spectrometry, traditional Chinese medicine, ultra-high-pressure liquid chromatography (UHPLC)

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